U.S. patent number 11,009,829 [Application Number 16/509,590] was granted by the patent office on 2021-05-18 for dual image storage material as well as preparation method and application thereof.
This patent grant is currently assigned to HUAZHONG UNIVERSITY OF SCIENCE AND TECHNOLOGY, HUAZHONG UNIVERSITY OF SCIENCE AND TECHNOLOGY. The grantee listed for this patent is Huazhong University of Science and Technology, Huazhong University of Science and Technology. Invention is credited to Haiyan Peng, Xiaolin Xie, Xiaoyu Zhao, Ye Zhao, Xingping Zhou.
United States Patent |
11,009,829 |
Peng , et al. |
May 18, 2021 |
Dual image storage material as well as preparation method and
application thereof
Abstract
The disclosure belongs to the technical field of photopolymer
materials, and more particularly relates to a dual image storage
material as well as a preparation method and application thereof.
The dual image storage material is obtained by selective
photoreaction of 1 to 50 parts by weight of an organic fluorescent
material, 7 to 50 parts by weight of liquid crystal, 0.2 to 10
parts by weight of a photoinitiator and 33 to 67 parts by weight of
photopolymerizable monomers. The obtained dual image storage
material can present a high-brightness holographic pattern under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position. The presented holographic and fluorescent
patterns may be the same or different. The obtained dual image
storage material can be used in the field of optical
anti-counterfeiting, optical information storage, displays or the
like.
Inventors: |
Peng; Haiyan (Hubei,
CN), Zhao; Ye (Hubei, CN), Xie; Xiaolin
(Hubei, CN), Zhou; Xingping (Hubei, CN),
Zhao; Xiaoyu (Hubei, CN) |
Applicant: |
Name |
City |
State |
Country |
Type |
Huazhong University of Science and Technology |
Hubei |
N/A |
CN |
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Assignee: |
HUAZHONG UNIVERSITY OF SCIENCE AND
TECHNOLOGY (Hubei, CN)
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Family
ID: |
68614566 |
Appl.
No.: |
16/509,590 |
Filed: |
July 12, 2019 |
Prior Publication Data
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Document
Identifier |
Publication Date |
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US 20190361393 A1 |
Nov 28, 2019 |
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Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
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PCT/CN2018/094930 |
Jul 9, 2018 |
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Foreign Application Priority Data
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May 23, 2018 [CN] |
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201810503543.3 |
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Current U.S.
Class: |
1/1 |
Current CPC
Class: |
G03H
1/02 (20130101); G03H 1/0011 (20130101); C09K
11/06 (20130101); G11B 7/24044 (20130101); G11B
7/245 (20130101); G03H 2260/12 (20130101); C09K
2211/1018 (20130101); G03H 2001/0264 (20130101); G11B
2007/24624 (20130101); C09K 2211/1007 (20130101); C09K
2211/1011 (20130101) |
Current International
Class: |
G03H
1/02 (20060101); G03H 1/18 (20060101); C09K
11/06 (20060101); G03H 1/00 (20060101) |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
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101329546 |
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Dec 2008 |
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CN |
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106950744 |
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Jul 2017 |
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CN |
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Other References
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examiner.
|
Primary Examiner: Angebranndt; Martin J
Attorney, Agent or Firm: Hamre, Schumann, Mueller &
Larson, P.C.
Claims
What is claimed is:
1. A dual image storage material, wherein the dual image storage
material is obtained by selective photoreaction of a composition
comprising: an organic fluorescent material, a liquid crystal, a
photoinitiator, and a photopolymerizable monomer, wherein the
photopolymerizable monomer is a mixture of a monofunctional monomer
and a polyfunctional monomer, the monofunctional monomer has a
single carbon-carbon double bond, and the polyfunctional monomer
has multiple carbon-carbon double bonds, the organic fluorescent
material includes one or more compounds selected from the group
consisting of substituted 1,1,2,2-tetraphenylethene (TPE),
substituted 1,1,2,3,4,5-pentaphenyl-1H-pyrrole, substituted
1,1,2,3,4,5-hexaphenyl-1H-silole (HPS), substituted
9,10-di[(E)-styryl]anthracene (DSA), substituted
10,10',11,11'-tetrahydro-5,5'-bidibenzo[a,d][7]annulenylidene
(THBA), substituted benzhydrylidenefluorene, and substituted
2,2'-(2,6-diphenylanthracene-9,10-diylidene)dimalononitrile (PDAB),
##STR00005## ##STR00006## where the substituent groups R in the
structural formulae are each independently selected from the group
consisting of n-hexyl, n-amyl, citronellol group,
4'-heptyl-4-biphenylcarbonitrile,
4'-(octyloxy)-4-biphenylcarbonitrile, 4-cyano-4'-pentylbiphenyl,
and 4-butoxy-[1,1'-biphenyl]-4'-carbonitrile.
2. The dual image storage material according to claim 1, wherein
the dual image storage material is obtained by selective
photoreaction of 1 to 50 parts by weight of the organic fluorescent
material, 7 to 50 parts by weight of the liquid crystal, 0.2 to 10
parts by weight of the photoinitiator and 33 to 67 parts by weight
of the photopolymerizable monomer.
3. The dual image storage material according to claim 2, wherein
the monofunctional monomer and the polyfunctional monomer are mixed
in a mass ratio of 3:1 to 1:2; the monofunctional monomer comprises
one or more of N,N-dimethylacrylamide, 2-hydroxyethyl acrylate,
2-hydroxyethyl methacrylate, acrylic acid, and methacrylic acid;
and the polyfunctional monomer comprises one or more of ethylene
dimethacrylate, pentaerythritol triacrylate, pentaerythritol
tetraacrylate, and hyperbranched acrylate.
4. The dual image storage material according to claim 2, wherein
the liquid crystal is one or more of
4'-heptyl-4-biphenylcarbonitrile, 4-cyano-4'-pentylbiphenyl,
4'-(octyloxy)-4-biphenylcarbonitrile,
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile, biphenylcyanogen liquid
crystal mixture E7 and biphenylcyanogen liquid crystal mixture
P0616A.
5. The dual image storage material according to claim 2, wherein
the photoinitiator is an ultraviolet initiator or a visible light
initiator or a combination thereof; the visible light initiator is
bis(2,6-difluoro-3-(1-hydropyrrol-1-yl)phenyl)titanocene, a mixture
of 3,3'-carbonylbis(7-diethylaminocoumarin) and N-phenylglycine, or
a mixture of Rose Bengal disodium salt and N-phenylglycine; and the
ultraviolet initiator is a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone.
6. The dual image storage material according to claim 1, wherein
the photoinitiator is a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone.
7. The dual image storage material according to claim 1, wherein
the photoinitiator includes an ultraviolet initiator and a visible
light initiator, the visible light initiator is
bis(2,6-difluoro-3-(1-hydropyrrolo-1-yl)phenyl)titanocene, a
mixture of 3,3'-carbonylbis(7-diethylaminocoumarin) and
N-phenylglycine, or a mixture of Rose Bengal disodium salt and
N-phenylglycine; and the ultraviolet initiator is a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone.
8. A preparation method for the dual image storage material
according to claim 1, comprising: (1) uniformly mixing 1 to 50
parts by weight of the organic fluorescent material, 7 to 50 parts
by weight of the liquid crystal, 0.2 to 10 parts by weight of the
photoinitiator and 33 to 67 parts by weight of the
photopolymerizable monomer to obtain a precursor of the dual image
storage material; (2) packaging the precursor of the dual image
storage material obtained in the step (1) in a liquid crystal cell,
and irradiating it with a coherent laser to cause free radical
polymerization of the photopolymerizable monomer, thereby obtaining
a holographic material in which a hologram image is stored; (3)
irradiating the holographic material obtained in the step (2) with
ultraviolet light through a mask to obtain a dual image storage
material in which a holographic material and a fluorescence image
are both stored, the mask being used for defining a pattern of the
fluorescent image; (4) postcuring the dual image storage material
obtained in the step (3) by visible light or ultraviolet light to
completely react the remaining photopolymerizable monomer so as to
fix the images.
9. The preparation method according to claim 8, wherein the
coherent laser in the step (2) has a wavelength of 432 to 633
nanometer and an irradiation time of 10 to 50 seconds.
10. The preparation method according to claim 8, wherein the
ultraviolet light in the step (3) has a wavelength of 200 to 370
nanometer, an irradiation intensity of 10 to 200 milliwatts per
square centimeter and an irradiation time of 2 to 60 minutes.
11. A method of forming a holographic/fluorescent dual pattern for
optical anti-counterfeiting or optical information storage or
display, comprising, obtaining the dual image storage material of
claim 1 by holographically recording a two-dimensional holographic
pattern or a three-dimensional holographic pattern and subsequently
using a masked exposure to record a two dimensional fluorescent
image, wherein the two-dimensional holographic pattern or
three-dimensional holographic pattern or two-dimensional
fluorescent image is visible to a naked eye under sunlight or
ultraviolet light.
Description
BACKGROUND
Technical Field
The present disclosure belongs to the technical field of
photopolymer materials, and more particularly relates to a dual
image storage material as well as a preparation method and
application thereof.
Description of the Related Art
Amorphous Alloys have,
Image storage is widely used in optical anti-counterfeiting,
optical information storage, displays and other fields. Holographic
technology is an effective means of image storage. The basic
principle of the holographic technology is that two coherent lasers
in space interfere with each other to form a grating, and both
amplitude and phase information of the coherent lasers are recorded
to realize three-dimensional (3D) information storage. The
holographic technology can also record two-dimensional (2D) images.
The holographic technology is not only widely used in data storage,
distributed feedback lasers, sensors and other fields, but also
plays an important role in high-end optical anti-counterfeiting
since the recorded images have the characteristics of good visual
effects, significant public recognition capabilities, difficult
counterfeiting techniques and the like.
In the field of anti-counterfeiting, with the development of
technology, the existing technologies face great challenges. In
order to improve the security and monopoly of anti-counterfeiting,
the development of multi-functional anti-counterfeiting technology
is an effective way. Combining the holographic technology with
other related disciplines to improve the anti-counterfeiting
performance has become a development direction of
anti-counterfeiting technology.
Optical anti-counterfeiting has the characteristic of easy
identification and is the most powerful anti-counterfeiting means.
Combining the holographic technology with fluorescent display
technology to display two images in the same spatial position but
under different conditions can realize the organic unity of overt
anti-counterfeiting and covert anti-counterfeiting, and effectively
improve the anti-counterfeiting ability. However, most organic
fluorescent materials have an aggregation-caused quenching (ACQ)
effect, that is, they exhibit a significant decrease in
fluorescence brightness in a solid state. At present, there is a
lack of effective dual optical anti-counterfeit image (holographic
image and fluorescent image) storage materials.
SUMMARY
In view of the above-described defects or improvement requirements
in the art, the present disclosure provides a dual image storage
material as well as a preparation method and application thereof,
and aims to provide a dual image storage material, which realizes
independent display of a holographic image and a fluorescent image
in the same space but under different illuminations, thereby
improving the security and monopoly of anti-counterfeiting
technology.
In order to achieve the above objective, according to an aspect of
the present disclosure, there is provided a dual image storage
material, in which in the same spatial position of the dual image
storage material, a holographic pattern visible to the naked eyes
is presented under sunlight, and a fluorescent pattern is presented
under ultraviolet light, the holographic pattern being a
two-dimensional image or a three-dimensional image.
Preferably, the dual image storage material is obtained by
selective photoreaction of 1 to 50 parts by weight of an organic
fluorescent material, 7 to 50 parts by weight of liquid crystal,
0.2 to 10 parts by weight of a photoinitiator and 33 to 67 parts by
weight of photopolymerizable monomers.
Preferably, the photopolymerizable monomers are a mixture of
monofunctional monomers and polyfunctional monomers in a mass ratio
of 3:1 to 1:2; the monofunctional monomers are one or more of
N,N-dimethylacrylamide, 2-hydroxyethyl acrylate, 2-hydroxyethyl
methacrylate, acrylic acid and methacrylic acid; and the
polyfunctional monomers are one or more of ethylene dimethacrylate,
pentaerythritol triacrylate, pentaerythritol tetraacrylate, and
hyperbranched acrylate.
Preferably, the organic fluorescent material is one or more of
substituted 1,1,2,2-tetraphenylethene (TPE), substituted
1,2,3,4,5-pentaphenyl-1H-pyrrole, substituted
1,1,2,3,4,5-hexaphenyl-1H-silole (HPS), substituted
10,10',11,11'-tetrahydro-5,5'-bidibenzo[a,d][7]annulenylidene
(THBA), substituted 9,10-di[(E)-styryl]anthracene (DSA),
substituted
2,2'-(2,6-diphenylanthracene-9,10-diylidene)dimalononitrile (PDAB)
and substituted benzhydrylidenefluorene, structural formulae of
which are shown as follows:
##STR00001## ##STR00002## where substituent groups R in the
structural formulae of the organic fluorescent material are each
independently selected from the group consisting of n-hexyl,
n-amyl, citronellol group, 4'-heptyl-4-biphenylcarbonitrile,
4'-(octyloxy)-4-biphenylcarbonitrile, 4-cyano-4'-pentylbiphenyl,
and 4-butoxy-[1,1'-biphenyl]-4'-carbonitrile.
Preferably, the liquid crystal is one or more of
4'-heptyl-4-biphenylcarbonitrile (7CB), 4-cyano-4'-pentylbiphenyl
(5CB), 4'-(octyloxy)-4-biphenylcarbonitrile (8OCB),
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (4OCB), biphenylcyanogen
liquid crystal mixture E7 and biphenylcyanogen liquid crystal
mixture P0616A.
Preferably, the photoinitiator is an ultraviolet initiator or a
visible light initiator; the visible light initiator is
bis(2,6-difluoro-3-(1-hydropyrrolo-1-yl)phenyl)titanocene, a
mixture of 3,3'-carbonylbis(7-diethylaminocoumarin) and
N-phenylglycine, or a mixture of acid red 94 (Rose Bengal disodium
salt) and N-phenylglycine; and the ultraviolet initiator is a
mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone.
According to another aspect of the present disclosure, there is
provided a preparation method for the dual image storage material,
comprising: (1) uniformly mixing 1 to 50 parts by weight of an
organic fluorescent material, 7 to 50 parts by weight of liquid
crystal, 0.2 to 10 parts by weight of a photoinitiator and 33 to 67
parts by weight of photopolymerizable monomers to obtain a
precursor of the dual image storage material; (2) packaging the
precursor of the dual image storage material obtained in the step
(1) in a liquid crystal cell, and irradiating it with a coherent
laser to cause free radical polymerization of the
photopolymerizable monomers, thereby obtaining a holographic
material in which a hologram image is stored; (3) irradiating the
holographic material obtained in the step (2) with ultraviolet
light through a mask to obtain a dual image storage material in
which a holographic material and a fluorescence image are both
stored, the mask being used for defining a pattern of the
fluorescent image; (4) postcuring the dual image storage material
obtained in the step (3) by visible light or ultraviolet light to
completely react the remaining photopolymerizable monomers so as to
fix the images.
Preferably, the mixing in the step (1) specifically includes:
performing a magnetic stirring or ultrasonic operation for 5 to 60
minutes at a temperature of 20 to 90 degrees Celsius.
Preferably, the coherent laser in the step (2) has a wavelength of
432 to 633 nanometer and an irradiation time of 10 to 50
seconds.
Preferably, the ultraviolet light in the step (3) has a wavelength
of 200 to 370 nanometer, an irradiation intensity of 10 to 200
milliwatts per square centimeter, and an irradiation time of 2 to
60 minutes.
Preferably, the post-cure time in the step (4) is 5 to 60
minutes.
According to another aspect of the present disclosure, there is
provided use of the dual image storage material in the field of
optical anti-counterfeiting, optical information storage or
displays
In general, by comparing the above technical solution of the
present inventive concept with the prior art, the present
disclosure has the following beneficial effects.
The present disclosure successfully combines the holographic
technology with fluorescent display technology to display two
images in the same spatial position but under different conditions,
thereby achieving the organic unity of overt anti-counterfeiting
and covert anti-counterfeiting and effectively improving the
anti-counterfeiting ability.
In the present disclosure, an organic fluorescent material having
aggregation-induced luminescence properties is introduced and the
organic fluorescent material is modified with a specific group,
thereby effectively solving the influence of the introduction of a
large amount of organic fluorescent material on the degree of phase
separation and the modulation degree of refractive index in the
holographic system. The technical solution can achieve high
brightness and high contrast of the fluorescent pattern, and can
also ensure that the brightness of the holographic image is not
affected. The independent coexistence of the holographic image and
the fluorescent image is realized, thereby achieving the storage of
the dual images.
The dual image storage according to the invention not only has an
important application in the field of high-end optical
anti-counterfeiting, but also can be applied to the fields of
optical information storage, displays and the like.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a holographic image obtained in Embodiment 6 of the
present disclosure;
FIG. 2 is a fluorescent image obtained in Embodiment 6 of the
present disclosure.
DETAILED DESCRIPTION OF THE EMBODIMENTS
For clear understanding of the objectives, features and advantages
of the present disclosure, detailed description of the present
disclosure will be given below in conjunction with accompanying
drawings and specific embodiments. It should be noted that the
embodiments described herein are only meant to explain the present
disclosure, and not to limit the scope of the present disclosure.
Furthermore, the technical features related to the embodiments of
the present disclosure described below can be mutually combined if
they are not found to be mutually exclusive.
Optical anti-counterfeiting has the characteristic of easy
identification and is the most powerful anti-counterfeiting means.
Combining holographic technology with fluorescent display
technology to display two images in the same spatial position but
under different conditions can realize the organic unity of overt
anti-counterfeiting and covert anti-counterfeiting, and effectively
improve the anti-counterfeiting ability. However, most organic
fluorescent materials have an aggregation-caused quenching (ACQ)
effect, that is, they exhibit a significant decrease in
fluorescence brightness in a solid state. In order to ensure the
brightness and contrast of the fluorescent image, a large amount of
organic fluorescent material needs to be introduced into the
holographic system, and the organic photochromic material is a good
choice. However, since the organic fluorescent material has poor
diffusibility and its refractive index cannot match the
photopolymerizable monomer or liquid crystal in the holographic
material (especially when the content of the fluorescent material
is increased to a certain extent, good diffusion performance is
more important), the introduction of a large amount of organic
fluorescent material may have a large influence on the degree of
phase separation and the modulation degree of refractive index in
the holographic system, resulting in a decrease in the brightness
of the hologram. Therefore, it is still a challenge to combine the
holographic technology with the fluorescent display technology to
increase the brightness and contrast of the fluorescent image
without reducing the brightness of the hologram.
In the present disclosure, by introducing an organic photochromic
fluorescent material and modifying a functional unit of the organic
fluorescent material with a certain substituent, the modified
organic fluorescent material can be mutually soluble with the
liquid crystal in the holographic system, so that when the
holographic image is formed, the micromolecular organic fluorescent
material enters the liquid crystal phase with the liquid crystal
micromolecules, and thus the problem of diffusion of a small amount
of organic fluorescent material in the holographic system is better
solved. Therefore, a small amount of organic fluorescent material
can also make the fluorescent image have sufficient brightness,
thereby achieving independent coexistence of the holographic image
and the fluorescent image, and achieving the storage of the dual
images.
The dual image storage material according to the present disclosure
is obtained by selective photoreaction of 1 to 50 parts by weight
of an organic fluorescent material, 7 to 50 parts by weight of
liquid crystal, 0.2 to 10 parts by weight of a photoinitiator and
33 to 67 parts by weight of photopolymerizable monomers. In the
selective photoreaction, 7 to 50 parts by weight of liquid crystal,
0.2 to 10 parts by weight of a photoinitiator and 33 to 67 parts by
weight of photopolymerizable monomers are irradiated by a coherent
laser to cause free radical polymerization of the
photopolymerizable monomers so as to obtain a holographic material
in which a hologram image is stored. In addition, in the selective
photoreaction, the organic fluorescent material is irradiated by
ultraviolet light to obtain an image storage material in which a
fluorescent pattern is stored.
The present disclosure provides a preferred dual image storage
material, which is obtained by selective photoreaction of 1 to 50
parts by weight of an organic fluorescent material, 7 to 50 parts
by weight of liquid crystal, 0.2 to 10 parts by weight of a
photoinitiator and the balance of photopolymerizable monomers.
The photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 3:1 to 1:2;
the monofunctional monomers are one or more of
N,N-dimethylacrylamide, 2-hydroxyethyl acrylate, 2-hydroxyethyl
methacrylate, acrylic acid and methacrylic acid; and the
polyfunctional monomers are one or more of ethylene dimethacrylate,
pentaerythritol triacrylate, pentaerythritol tetraacrylate, and
hyperbranched acrylate.
The organic fluorescent material is one or more of substituted TPE,
substituted 1,2,3,4,5-pentaphenyl-1H-pyrrole, substituted HPS,
substituted THBA, substituted DSA, substituted PDAB, and
substituted benzhydrylidenefluorene, structural formulae of which
are shown as follows. The benzene rings of the organic fluorescent
material contain at least one of the following substituent groups:
n-hexyl, n-amyl, citronellol group,
4'-heptyl-4-biphenylcarbonitrile (7CB),
4'-(octyloxy)-4-biphenylcarbonitrile (8OCB),
4-cyano-4'-pentylbiphenyl (5CB) and
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (4OCB). A typical organic
fluorescent material has the following structural general formula,
and in the formula, the R group is independently selected from the
group consisting of n-hexyl, n-amyl, citronellol group,
4'-heptyl-4-biphenylcarbonitrile (7CB),
4'-(octyloxy)-4-biphenylcarbonitrile (8OCB),
4-cyano-4'-pentylbiphenyl (5CB) and
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (4OCB). Organic
fluorescent materials having these general formulae can be obtained
by conventional synthesis and modification means.
##STR00003## ##STR00004##
The liquid crystal is one or more of
4'-heptyl-4-biphenylcarbonitrile (7CB), 4-cyano-4'-pentylbiphenyl
(5CB), 4'-(octyloxy)-4-biphenylcarbonitrile (8OCB),
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (4OCB), biphenylcyanogen
liquid crystal mixture E7 and biphenylcyanogen liquid crystal
mixture P0616A.
The photoinitiator is an ultraviolet initiator or a visible light
initiator. The visible light initiator is a mixture of
3,3'-carbonylbis(7-diethylaminocoumarin) and anilinoacetic acid, a
mixture of acid red 94 and anilinoacetic acid, or
bis(2,6-difluoro-3-(1-hydropyrrol-1-yl)phenyl)titanocene. The
ultraviolet initiator is a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone.
A preparation method for the dual image storage material according
to the present disclosure comprises:
(1) Uniformly mixing 1 to 50 parts by weight of an organic
fluorescent material, 7 to 50 parts by weight of liquid crystal,
0.2 to 10 parts by weight of a photoinitiator and 33 to 67 parts by
weight of photopolymerizable monomers to obtain a precursor of the
dual image storage material.
In the above step, the specific mass fractions of the
monofunctional monomers and the polyfunctional monomers are
determined according to the molecular weight of the above monomer
and the number of carbon-carbon double bonds contained in the
compound; the optimum mass fractions are such that the
monofunctional monomers and the polyfunctional monomers have
approximately the same number of carbon-carbon double bonds.
The photoinitiator is a photoinitiator suitable for the free
radical polymerization of coherent laser excitation in step (2),
for example, 3,3'-carbonylbis(7-diethylaminecoumarin) and
anilinoacetic acid a mixture having a mass ratio of 1:5 to 5:1 or
bis(2,6-difluoro-3-(1-hydropyrrol-1-yl)phenyl)titanocene
The method of uniformly mixing includes: performing a magnetic
stirring or ultrasonic operation for 5 to 60 minutes at a
temperature of 20 to 90 degrees Celsius.
(2) Packaging the precursor of the dual image storage material
obtained in the step (1) in a liquid crystal cell, and irradiating
it with a coherent laser of 432 to 633 nanometer for 10 to 50
seconds to cause free radical polymerization of the monofunctional
monomers and the polyfunctional monomers, thereby obtaining a
holographic material in which a hologram image is stored. The
principle of holographic imaging is that a laser beam produces two
beams of coherent homologous light through a beam splitter, and one
of the two beams of homologous coherent light illuminates an object
to produce diffusely reflected light (referred to as object light),
which then interferes with another beam of homologous laser
(referred to as reference light) to form a grating, so that both
phase and amplitude information of the coherent lights are recorded
on the recording medium (the precursor of the dual image storage
material) to realize 3D holographic information storage.
(3) Irradiating the holographic material obtained in the step (2)
with ultraviolet light through a mask to obtain a dual image
storage material in which a holographic image and a fluorescence
image are both stored, in which the ultraviolet light has an
irradiation time of 2 to 60 minutes, a light intensity of 10 to 200
milliwatts per square centimeter and a wavelength of 200 to 370
nanometer. The mask is used for defining a pattern of the
fluorescent image, and is made of two materials, one of which
(e.g., soda glass) passes ultraviolet light and another of which
(e.g., metal) does not pass ultraviolet light, and a metal material
is used on the mask to form a desired pattern, that is, a
fluorescent pattern. When the holographic material is irradiated by
the ultraviolet light through the mask, the ultraviolet light
passing through the glass portion of the mask irradiates into the
holographic material and the fluorescence of the organic
fluorescent material irradiated by the ultraviolet light is
quenched. Since the ultraviolet light cannot penetrate the metal
material, the fluorescence of a part of the organic fluorescent
material in the holographic material is not quenched, and the
corresponding pattern is the same as that of the metal material on
the mask, that is, the fluorescent pattern.
(4) Postcuring the dual image storage material obtained in the step
(3) by visible light or ultraviolet light to completely react the
remaining photopolymerizable monomers so as to fix the images. The
visible light or ultraviolet light has an irradiation time of 5 to
60 minutes.
The dual image storage material according to the present disclosure
has the characteristics of double anti-counterfeiting, high pattern
contrast and simple fabrication. The source used has a wavelength
of 432 to 633 nanometer, preferably 532 nanometer. The ultraviolet
light used has a wavelength of 200 to 370 nanometer, preferably 300
nanometer.
When the dual image storage material according to the present
disclosure is used for double anti-counterfeiting, in a case where
the image storage material is irradiated with visible light, a
holographic image may be presented, and in a case where the image
storage material is irradiated with ultraviolet light, according to
the light stimuli responsiveness of the organic fluorescent
material, a fluorescent pattern determined in advance by the mask
pattern in the image storage material can be observed through the
naked eye.
Embodiments are described below.
Comparative Example 1
In the present comparative example, the image storage material was
obtained by selective photoreaction of 1 parts by weight of an
organic fluorescent material (TPE, R group is hydrogen atom), 50
parts by weight of liquid crystal
(4'-heptyl-4-biphenylcarbonitrile, 7CB), 0.2 parts by weight of a
photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photoinitiator is an ultraviolet initiator which is a mixture
of bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone. The photopolymerizable
monomers is a mixture of monofunctional monomers
(N,N-dimethylacrylamide) and polyfunctional monomers (ethylene
dimethacrylate) in a mass ratio of 3:1.
A preparation method for the image storage material is as
follows.
First, TPE was added to a mixed solution of monomers and liquid
crystal (4'-heptyl-4-biphenylcarbonitrile, 7CB), a photoinitiator
(a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) was added to the solution, and
then ultrasonic dispersion was performed at 20 degrees Celsius for
60 minutes, so that the photoinitiator and the organic fluorescent
material were uniformly dispersed in the mixed solution of the
monomers and the liquid crystal to obtain a precursor of a dual
image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 432 nanometer for 10 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for 2
minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 200 nanometer and a
light intensity of 10 milliwatts per square centimeter. Finally,
the obtained image storage material was cured by irradiating it
with ultraviolet light for 5 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
In the present comparative example, since the unmodified organic
fluorescent material TPE was used, the organic fluorescent material
and the holographic system were not mutually soluble, resulting in
failure to obtain clear fluorescent and holographic images.
Embodiment 1
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 3 parts by weight of an organic fluorescent
material (1,2,3,4,5-pentaphenyl-1H-pyrrole, the R group is
n-hexyl), 48 parts by weight of liquid crystal
(4-cyano-4'-pentylbiphenyl, 5CB), 0.4 parts by weight of a
photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photoinitiator is a visible light initiator which is a mixture
of 3,3'-carbonylbis(7-diethylaminecoumarin) and anilinoacetic acid.
The photopolymerizable monomers are a mixture of monofunctional
monomers (2-hydroxyethyl acrylate) and polyfunctional monomers
(pentaerythritol triacrylate) in a mass ratio of 3:1.
A preparation method for the image storage material is as
follows.
First, 1,2,3,4,5-pentaphenyl-1H-pyrrole was added to a mixed
solution of monomers and liquid crystal (4-cyano-4'-pentylbiphenyl,
5CB), a photoinitiator (a mixture of
3,3'-carbonylbis(7-diethylaminecoumarin) and anilinoacetic acid)
was added to the solution, and then ultrasonic dispersion was
performed at 25 degrees Celsius for 57 minutes, so that the
photoinitiator and the organic fluorescent material are uniformly
dispersed in the mixed solution of the monomers and the liquid
crystal to obtain a precursor of a dual image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 441 nanometer for 15 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for 4
minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 211 nanometer and a
light intensity of 20 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 10 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 2
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 5 parts by weight of an organic fluorescent
material (HPS, the R group is n-amyl), 46 parts by weight of liquid
crystal (4'-(octyloxy)-4-biphenylcarbonitrile, 8OCB), 0.6 parts by
weight of a photoinitiator and 49 parts by weight of
photopolymerizable monomers.
The photoinitiator is an ultraviolet initiator which is a mixture
of bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone. The photopolymerizable
monomers are a mixture of monofunctional monomers (2-hydroxyethyl
methacrylate) and polyfunctional monomers (pentaerythritol
tetraacrylate) in a mass ratio of 2:1.
A preparation method for the image storage material is as
follows.
First, HPS was added to a mixed solution of monomers and liquid
crystal (4'-(octyloxy)-4-biphenylcarbonitrile, 8OCB), a
photoinitiator (a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) was added to the solution, and
then ultrasonic dispersion was performed at 30 degrees Celsius for
54 minutes, so that the photoinitiator and the organic fluorescent
material are uniformly dispersed in the mixed solution of the
monomers and the liquid crystal to obtain a precursor of a dual
image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 456 nanometer for 20 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for 6
minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 223 nanometer and a
light intensity of 30 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 15 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 3
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 7 parts by weight of an organic fluorescent
material (THBA, the R group is citronellol group), 44 parts by
weight of liquid crystal (4-butoxy-[1,1'-biphenyl]-4'-carbonitrile,
4OCB), 0.8 parts by weight of a photoinitiator and 49 parts by
weight of photopolymerizable monomers.
The photoinitiator is a visible light initiator which is a mixture
of acid red 94 and anilinoacetic acid. The photopolymerizable
monomers are a mixture of monofunctional monomers (acrylic acid)
and polyfunctional monomers (hyperbranched acrylate) in a mass
ratio of 12:7.
A preparation method for the image storage material is as
follows.
First, THBA was added to a mixed solution of monomers and liquid
crystal (4-butoxy-[1,1'-biphenyl]-4'-carbonitrile, 4OCB), a
photoinitiator (a mixture of acid red 94 and anilinoacetic acid)
was added to the solution, and then ultrasonic dispersion was
performed at 35 degrees Celsius for 51 minutes, so that the
photoinitiator and the organic fluorescent material are uniformly
dispersed in the mixed solution of the monomers and the liquid
crystal to obtain a precursor of a dual image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 462 nanometer for 25 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for 8
minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 245 nanometer and a
light intensity of 40 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 20 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 4
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 9 parts by weight of an organic fluorescent
material (DSA, the R group is 4'-heptyl-4-biphenylcarbonitrile
(7CB)), 42 parts by weight of liquid crystal
(4'-(octyloxy)-4-biphenylcarbonitrile, 8OCB), 1.0 parts by weight
of a photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photoinitiator is an ultraviolet initiator which is a mixture
of bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone. The photopolymerizable
monomers are a mixture of monofunctional monomers (2-hydroxyethyl
methacrylate) and polyfunctional monomers in a mass ratio of
3:2.
The polyfunctional monomers are a mixture of ethylene
dimethacrylate and pentaerythritol triacrylate.
A preparation method for the image storage material is as
follows.
First, DSA was added to a mixed solution of monomers and liquid
crystal (4'-(octyloxy)-4-biphenylcarbonitrile, 8OCB), a
photoinitiator (a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) was added to the solution, and
then ultrasonic dispersion was performed at 40 degrees Celsius for
48 minutes, so that the photoinitiator and the organic fluorescent
material are uniformly dispersed in the mixed solution of the
monomers and the liquid crystal to obtain a precursor of a dual
image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 478 nanometer for 30 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
10 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 254 nanometer and a
light intensity of 50 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 25 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 5
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 11 parts by weight of an organic fluorescent
material (PDAB, the R group is 4'-(octyloxy)-4-biphenylcarbonitrile
(8OCB)), 40 parts by weight of biphenylcyanogen liquid crystal
mixture (P0616A), 1.2 parts by weight of a photoinitiator and 49
parts by weight of photopolymerizable monomers.
The photoinitiator is a visible light initiator which is
bis(2,6-difluoro-3-(1-hydropyrrol-1-yl)phenyl)titanocene. The
photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 4:3.
The monofunctional monomers are a mixture of N,N-dimethylacrylamide
and 2-hydroxyethyl acrylate. The polyfunctional monomers are a
mixture of ethylene dimethacrylate and pentaerythritol
tetraacrylate.
A preparation method for the image storage material is as
follows.
First, PDAB was added to a mixed solution of monomers and P0616A, a
photoinitiator
(bis(2,6-difluoro-3-(1-hydropyrrol-1-yl)phenyl)titanocene) was
added to the solution, and then ultrasonic dispersion was performed
at 45 degrees Celsius for 45 minutes, so that the photoinitiator
and the organic fluorescent material are uniformly dispersed in the
mixed solution of the monomers and the liquid crystal to obtain a
precursor of a dual image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 495 nanometer for 35 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
12 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 266 nanometer and a
light intensity of 50 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 30 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 6
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 13 parts by weight of an organic fluorescent
material (benzhydrylidenefluorene, the R group is
4-cyano-4'-pentylbiphenyl (5CB)), 38 parts by weight of liquid
crystal, 1.4 parts by weight of a photoinitiator and 49 parts by
weight of photopolymerizable monomers.
The liquid crystal is a mixture of 4'-heptyl-4-biphenylcarbonitrile
(7CB) and 4-cyano-4'-pentylbiphenyl (5CB).
The photoinitiator is an ultraviolet initiator which is a mixture
of bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone. The photopolymerizable
monomers are a mixture of monofunctional monomers and
polyfunctional monomers in a mass ratio of 6:5.
The monofunctional monomers are a mixture of N,N-dimethylacrylamide
and 2-hydroxyethyl methacrylate. The polyfunctional monomers are a
mixture of ethylene dimethacrylate and hyperbranched acrylate.
A preparation method for the image storage material is as
follows.
First, benzhydrylidenefluorene was added to a mixed solution of
monomers and liquid crystal, a photoinitiator (a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) was added to the solution, and
then ultrasonic dispersion was performed at 50 degrees Celsius for
42 minutes, so that the photoinitiator and the organic fluorescent
material are uniformly dispersed in the mixed solution of the
monomers and the liquid crystal to obtain a precursor of a dual
image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 503 nanometer for 40 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image (as shown in FIG. 1) is stored.
Subsequently, the holographic material was irradiated with
ultraviolet light through a mask for 14 minutes to obtain a dual
image storage material in which a holographic image and a
fluorescent pattern (as shown in FIG. 2) are both stored, in which
the ultraviolet light has a wavelength of 278 nanometer and a light
intensity of 70 milliwatts per square centimeter. Finally, the
obtained dual image storage material was cured by irradiating it
with ultraviolet light for 35 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
The holographic image is as shown in FIG. 1, and the fluorescent
pattern is as shown in FIG. 2.
Embodiment 7
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 15 parts by weight of an organic fluorescent
material, 36 parts by weight of liquid crystal, 0.6 parts by weight
of a photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 12:11. The
monofunctional monomers are a mixture of N,N-dimethylacrylamide and
acrylic acid. The polyfunctional monomers are a mixture of ethylene
dimethacrylate, pentaerythritol triacrylate and pentaerythritol
tetraacrylate.
The organic fluorescent material is a mixture of TPE and
1,2,3,4,5-pentaphenyl-1H-pyrrole, in which the R group is
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (4OCB).
The liquid crystal is a mixture of 4'-heptyl-4-biphenylcarbonitrile
(7CB) and 4'-(octyloxy)-4-biphenylcarbonitrile (8OCB).
The photoinitiator is a visible light initiator. The visible light
initiator is a mixture of 3,3'-carbonylbis(7-diethylaminecoumarin)
and anilinoacetic acid.
A preparation method for the image storage material is as
follows.
First, the organic fluorescent material was added to a mixed
solution of monomers and liquid crystal, a photoinitiator (a
mixture of 3,3'-carbonylbis(7-diethylaminecoumarin) and
anilinoacetic acid) was added to the solution, and then ultrasonic
dispersion was performed at 55 degrees Celsius for 39 minutes, so
that the photoinitiator and the organic fluorescent material are
uniformly dispersed in the mixed solution of the monomers and the
liquid crystal to obtain a precursor of a dual image storage
material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 512 nanometer for 45 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
16 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 288 nanometer and a
light intensity of 80 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 40 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 8
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 17 parts by weight of an organic fluorescent
material, 34 parts by weight of liquid crystal, 3 parts by weight
of a photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 1:1. The
monofunctional monomers are a mixture of N,N-dimethylacrylamide and
methacrylic acid. The polyfunctional monomers are a mixture of
ethylene dimethacrylate, pentaerythritol tetraacrylate, and
hyperbranched acrylate.
The organic fluorescent material is a mixture of TPE and HPS, in
which the R group is hydrogen atom and n-hexyl.
The liquid crystal is a mixture of 4'-heptyl-4-biphenylcarbonitrile
(7CB) and 4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (4OCB).
The photoinitiator is an ultraviolet initiator. The ultraviolet
initiator is a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone.
A preparation method for the image storage material is as
follows.
First, the organic fluorescent material was added to a mixed
solution of monomers and liquid crystal, a photoinitiator (a
mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone mixture) was added to the
solution, and then ultrasonic dispersion was performed at 60
degrees Celsius for 36 minutes, so that the photoinitiator and the
organic fluorescent material are uniformly dispersed in the mixed
solution of the monomers and the liquid crystal to obtain a
precursor of a dual image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 527 nanometer for 50 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
18 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 296 nanometer and a
light intensity of 90 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 45 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 9
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 19 parts by weight of an organic fluorescent
material, 32 parts by weight of liquid crystal, 4 parts by weight
of a photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 12:13. The
monofunctional monomers are a mixture of 2-hydroxyethyl acrylate
and 2-hydroxyethyl methacrylate. The polyfunctional monomers are a
mixture of ethylene dimethacrylate, hyperbranched acrylate, and
pentaerythritol triacrylate.
The organic fluorescent material is a mixture of TPE and THBA, in
which the R group is hydrogen atom and n-amyl.
The liquid crystal is a mixture of 4-cyano-4'-pentylbiphenyl (5CB)
and 4'-(octyloxy)-4-biphenylcarbonitrile (8OCB).
The photoinitiator is a visible light initiator. The visible light
initiator is a mixture of acid red 94 and anilinoacetic acid.
A preparation method for the image storage material is as
follows.
First, the organic fluorescent material was added to a mixed
solution of monomers and liquid crystal, a photoinitiator (a
mixture of acid red 94 and anilinoacetic acid) was added to the
solution, and then ultrasonic dispersion was performed at 65
degrees Celsius for 33 minutes, so that the photoinitiator and the
organic fluorescent material are uniformly dispersed in the mixed
solution of the monomers and the liquid crystal to obtain a
precursor of a dual image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 535 nanometer for 12 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
20 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 300 nanometer and a
light intensity of 100 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 50 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 10
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 21 parts by weight of an organic fluorescent
material, 30 parts by weight of liquid crystal, 5 parts by weight
of a photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 6:7. The
monofunctional monomers are a mixture of 2-hydroxyethyl acrylate
and acrylic acid. The polyfunctional monomers are a mixture of
pentaerythritol triacrylate, pentaerythritol tetraacrylate and
hyperbranched acrylate.
The organic fluorescent material is a mixture of TPE and DSA, in
which the R group is hydrogen atom and citronellol group.
The liquid crystal is a mixture of 4-cyano-4'-pentylbiphenyl (5CB)
and 4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (4OCB).
The photoinitiator is an ultraviolet initiator. The ultraviolet
initiator is a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone.
A preparation method for the image storage material is as
follows.
First, the organic fluorescent material was added to a mixed
solution of monomers and liquid crystal, a photoinitiator (a
mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) was added to the solution, and
then ultrasonic dispersion was performed at 70 degrees Celsius for
30 minutes, so that the photoinitiator and the organic fluorescent
material are uniformly dispersed in the mixed solution of the
monomers and the liquid crystal to obtain a precursor of a dual
image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 549 nanometer for 17 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
22 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 310 nanometer and a
light intensity of 110 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 55 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 11
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 23 parts by weight of an organic fluorescent
material, 28 parts by weight of liquid crystal, 6 parts by weight
of a photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 4:5. The
monofunctional monomers are a mixture of 2-hydroxyethyl acrylate
and methacrylic acid. The polyfunctional monomers are a mixture of
pentaerythritol triacrylate and pentaerythritol tetraacrylate.
The organic fluorescent material is a mixture of TPE and PDAB, in
which the R group is hydrogen atom and
4'-heptyl-4-biphenylcarbonitrile (7CB).
The liquid crystal is a mixture of
4'-(octyloxy)-4-biphenylcarbonitrile (8OCB) and
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (4OCB).
The photoinitiator is a visible light initiator. The visible light
initiator is
bis(2,6-difluoro-3-(1-hydropyrrol-1-yl)phenyl)titanocene.
A preparation method for the image storage material is as
follows.
First, the organic fluorescent material was added to a mixed
solution of monomers and liquid crystal, a photoinitiator
(bis(2,6-difluoro-3-(1-hydropyrrol-1-yl)phenyl)titanocene) was
added to the solution, and then ultrasonic dispersion was performed
at 75 degrees Celsius for 27 minutes, so that the photoinitiator
and the organic fluorescent material are uniformly dispersed in the
mixed solution of the monomers and the liquid crystal to obtain a
precursor of a dual image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 553 nanometer for 23 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
24 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 325 nanometer and a
light intensity of 120 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 60 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 12
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 25 parts by weight of an organic fluorescent
material, 26 parts by weight of liquid crystal, 7 parts by weight
of a photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 3:4. The
monofunctional monomers are a mixture of 2-hydroxyethyl
methacrylate and acrylic acid. The polyfunctional monomers are a
mixture of pentaerythritol triacrylate and hyperbranched
acrylate.
The organic fluorescent material is a mixture of TPE and
benzhydrylidenefluorene, in which the R group is hydrogen atom and
4'-(octyloxy)-4-biphenylcarbonitrile (8OCB).
The liquid crystal is 4'-heptyl-4-biphenylcarbonitrile (7CB).
The photoinitiator is an ultraviolet initiator. The ultraviolet
initiator is a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone.
A preparation method for the image storage material is as
follows.
First, the organic fluorescent material was added to a mixed
solution of monomers and liquid crystal, a photoinitiator (a
mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) was added to the solution, and
then ultrasonic dispersion was performed at 85 degrees Celsius for
24 minutes, so that the photoinitiator and the organic fluorescent
material are uniformly dispersed in the mixed solution of the
monomers and the liquid crystal to obtain a precursor of a dual
image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 560 nanometer for 28 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
26 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 334 nanometer and a
light intensity of 130 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 5 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 13
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 27 parts by weight of an organic fluorescent
material, 24 parts by weight of liquid crystal, 8 parts by weight
of a photoinitiator and 49 parts by weight of photopolymerizable
monomers.
The photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 12:17. The
monofunctional monomers are a mixture of 2-hydroxyethyl
methacrylate and methacrylic acid. The polyfunctional monomers are
a mixture of pentaerythritol tetraacrylate and hyperbranched
acrylate.
The organic fluorescent material is a mixture of
1,2,3,4,5-pentaphenyl-1H-pyrrole and HPS, in which the R group is
hydrogen atom and 4-cyano-4'-pentylbiphenyl (5CB).
The liquid crystal is 4-cyano-4'-pentylbiphenyl (5CB).
The photoinitiator is a visible light initiator. The visible light
initiator is a mixture of 3,3'-carbonylbis(7-diethylaminecoumarin)
and anilinoacetic acid.
A preparation method for the image storage material is as
follows.
First, the organic fluorescent material was added to a mixed
solution of monomers and liquid crystal, a photoinitiator (a
mixture of 3,3'-carbonylbis(7-diethylaminecoumarin) and
anilinoacetic acid) was added to the solution, and then ultrasonic
dispersion was performed at 85 degrees Celsius for 21 minutes, so
that the photoinitiator and the organic fluorescent material are
uniformly dispersed in the mixed solution of the monomers and the
liquid crystal to obtain a precursor of a dual image storage
material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 579 nanometer for 31 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
28 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 345 nanometer and a
light intensity of 140 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 10 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
Embodiment 14
The dual image storage material according to the present disclosure
can present a holographic pattern visible to the naked eyes under
sunlight and a fluorescent pattern under ultraviolet light in the
same spatial position of the material; the holographic pattern and
the fluorescent pattern can be the same or different; the
holographic pattern may be a two-dimensional image or a
three-dimensional image, which can be observed with the naked eyes
under sunlight.
The dual image storage material was obtained by selective
photoreaction of 50 parts by weight of an organic fluorescent
material, 7 parts by weight of liquid crystal, 10 parts by weight
of a photoinitiator and 43 parts by weight of photopolymerizable
monomers.
The photopolymerizable monomers are a mixture of monofunctional
monomers and polyfunctional monomers in a mass ratio of 1:2. The
monofunctional monomers are a mixture of acrylic acid and
methacrylic acid. The polyfunctional monomers are ethylene
dimethacrylate.
The organic fluorescent material is a mixture of
1,2,3,4,5-pentaphenyl-1H-pyrrole and THBA, in which the R group is
hydrogen atom and 4-butoxy-[1,1'-biphenyl]-4'-carbonitrile
(4OCB).
The liquid crystal is 4'-(octyloxy)-4-biphenylcarbonitrile
(8OCB).
The photoinitiator is an ultraviolet initiator. The ultraviolet
initiator is a mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone.
A preparation method for the image storage material is as
follows.
First, the organic fluorescent material was added to a mixed
solution of monomers and liquid crystal, a photoinitiator (a
mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) was added to the solution, and
then ultrasonic dispersion was performed at 90 degrees Celsius for
18 minutes, so that the photoinitiator and the organic fluorescent
material are uniformly dispersed in the mixed solution of the
monomers and the liquid crystal to obtain a precursor of a dual
image storage material.
The precursor of the dual image storage material was irradiated
with a coherent laser of 580 nanometer for 37 seconds to cause free
radical polymerization of the monofunctional monomers and the
polyfunctional monomers so as to obtain a holographic material in
which a holographic image is stored. Subsequently, the holographic
material was irradiated with ultraviolet light through a mask for
30 minutes to obtain a dual image storage material in which a
holographic image and a fluorescent pattern are both stored, in
which the ultraviolet light has a wavelength of 356 nanometer and a
light intensity of 150 milliwatts per square centimeter. Finally,
the obtained dual image storage material was cured by irradiating
it with ultraviolet light for 15 minutes to completely react the
remaining photopolymerizable monomers so as to fix the images.
TABLE-US-00001 TABLE 1 Formulations related to other exemplary
embodiments of the present disclosure Organic fluorescent
Photopolymerizable Photopolymerizable material Liquid crystal
Photoinitiator monomer monomer Embodiment (parts by weight) (parts
by weight) (parts by weight) (parts by weight) (ratio) 16 31 20 9
49 12:19 17 33 18 1.5 49 3:5 18 35 16 2.5 49 12:21 19 37 14 3.5 49
6:11 20 39 12 4.5 49 12:23 21 41 10 6.5 49 2:3 22 43 8 7.5 49 6:7
23 45 22 8.5 33 4:5 24 47 9 9.5 44 3:4 25 49 11 0.5 40 12:17 26 29
13 1.1 58 2:3 27 48 15 2.2 37 12:19 28 46 17 3.4 37 3:5 29 44 19
7.8 37 12:21 30 12 21 8.2 67 6:11 Embodiment Monofunctional monomer
Polyfunctional monomer 16 N,N-dimethylacrylamide, 2-hydroxyethyl
acrylate, Pentaerythritol triacrylate 2-hydroxyethyl methacrylate
17 N,N-dimethylacrylamide, 2-hydroxyethyl acrylate, Pentaerythritol
tetraacrylate Acrylic acid 18 N,N-dimethylacrylamide,
2-hydroxyethyl acrylate, Hyperbranched acrylate Methacrylic acid 19
N,N-dimethylacrylamide, 2-hydroxyethyl methacrylate, Ethylene
dimethacrylate, Pentaerythritol Acrylic acid triacrylate 20
N,N-dimethylacrylamide, 2-hydroxyethyl methacrylate, Ethylene
dimethacrylate, Pentaerythritol Methacrylic acid tetraacrylate 21
N,N-dimethylacrylamide, Acrylic acid, Methacrylic acid Ethylene
dimethacrylate, Hyperbranched acrylate 22 2-hydroxyethyl acrylate,
2-hydroxyethyl methacrylate, Ethylene dimethacrylate,
Pentaerythritol Acrylic acid triacrylate, Pentaerythritol
tetraacrylate 23 2-hydroxyethyl acrylate, 2-hydroxyethyl
methacrylate, Ethylene dimethacrylate, Pentaerythritol Methacrylic
acid tetraacrylate, Hyperbranched acrylate 24 2-hydroxyethyl
methacrylate, Acrylic acid, Methacrylic Ethylene dimethacrylate,
Hyperbranched acid acrylate, Pentaerythritol triacrylate 25
2-hydroxyethyl acrylate, Acrylic acid, Methacrylic acid
Pentaerythritol triacrylate, Pentaerythritol tetraacrylate,
Hyperbranched acrylate 26 N,N-dimethylacrylamide Pentaerythritol
triacrylate, Pentaerythritol tetraacrylate 27 2-hydroxyethyl
acrylate Pentaerythritol triacrylate, Hyperbranched acrylate 28
2-hydroxyethyl methacrylate Pentaerythritol tetraacrylate,
Hyperbranched acrylate 29 Acrylic acid Ethylene dimethacrylate 30
Methacrylic acid Pentaerythritol triacrylate Organic fluorescent
Embodiment material R group Liquid crystal 16
1,2,3,4,5-pentaphenyl-1H-pyrrole, N-hexyl, N-amyl
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile DSA (4OCB) 17
1,2,3,4,5-pentaphenyl-1H-pyrrole, N-hexyl, Citronellol group
Biphenylcyanogen liquid crystal mixture PDAB (E7) 18
1,2,3,4,5-pentaphenyl-1H-pyrrole, N-hexyl, Biphenylcyanogen liquid
crystal mixture Benzhydrylidenefluorene
4'-heptyl-4-biphenylcarbonitrile (P0616A) (7CB) 19 HPS, THBA
N-hexyl, 4'-heptyl-4-biphenylcarbonitrile (7CB),
4'-(octyloxy)-4-biphenylcarbonitrile 4-cyano-4'-pentylbiphenyl
(5CB) (8OCB) 20 HPS, DSA N-hexyl, 4'-heptyl-4-biphenylcarbonitrile
(7CB), 4-cyano-4'-pentylbiphenyl
4'-(octyloxy)-4-biphenylcarbonitrile (5CB) (8OCB) 21 HPS, PDAB
N-hexyl, 4'-heptyl-4-biphenylcarbonitrile (7CB),
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile
4-butoxy-[1,1'-biphenyl]-4'-car- bonitrile (4OCB) (4OCB) 22 HPS,
N-amyl, Citronellol group 4-cyano-4'-pentylbiphenyl (5CB),
Benzhydrylidenefluorene 4'-(octyloxy)-4-biphenylcarbonitrile (8OCB)
23 THBA, DSA N-amyl, 4-cyano-4'-pentylbiphenyl (5CB),
4'-heptyl-4-biphenylcarbonitrile
4-butoxy-[1,1'-biphenyl]-4'-carbonitril- e (7CB) (4OCB) 24 THBA,
PDAB N-amyl, 4'-(octyloxy)-4-biphenylcarbonitrile
4'-(octyloxy)-4-biphenylcarbonitrile (8OCB), (8OCB)
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (4OCB) 25 THBA, N-amyl,
Biphenylcyanogen liquid crystal mixture Benzhydrylidenefluorene
4-cyano-4'-pentylbiphenyl (E7) (5CB) 26 DSA, PDAB N-amyl,
Biphenylcyanogen liquid crystal mixture
4-butoxy-[1,1'-biphenyl]-4'-carbonitrile (P0616A) (4OCB) 27 DSA,
Citronellol group, Biphenylcyanogen liquid crystal mixture
Benzhydrylidenefluorene 4-cyano-4'-pentylbiphenyl (E7) (5CB) 28
PDAB, Citronellol group, Biphenylcyanogen liquid crystal mixture
Benzhydrylidenefluorene 4-butoxy-[1,1'-biphenyl]-4'-carbonitrile
(P0616A)- (4OCB) 29 TPE hydrogen atom
4'-heptyl-4-biphenylcarbonitrile (7CB) 30
1,2,3,4,5-pentaphenyl-1H-pyrrole N-hexyl 4-cyano-4'-pentylbiphenyl
(5CB) Embodiment Photoinitiator 16 Visible light initiator (mixture
of acid red 94 and anilinoacetic acid) 17 Ultraviolet initiator
(mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone 18 Visible light initiator
(bis(2,6-difluoro-3-(1-hydropyrrol-1-yl)phenyl)titanocene) 19
Ultraviolet initiator (mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) 20 Visible light initiator
(mixture of 3,3'-carbonylbis(7-diethylaminocoumarin)) and
anilinoacetic acid) 21 Ultraviolet initiator (mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) 22 Visible light initiator
(mixture of acid red 94 and anilinoacetic acid) 23 Ultraviolet
initiator (mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) 24 Visible light initiator
(bis(2,6-difluoro-3-(1-hydropyrrol-1-yl)phenyl)titanocene) 25
Ultraviolet initiator (mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) 26 Visible light initiator
(mixture of 3,3'-carbonylbis(7-diethylaminocoumarin)) and
anilinoacetic acid) 27 Ultraviolet initiator (mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) 28 Visible light initiator
(mixture of Acid red 94 and anilinoacetic acid) 29 Ultraviolet
initiator (mixture of
bis(2,6-dimethoxybenzoyl)(2,4,4-trimethylpentyl)-phosphine oxide
and 2-hydroxy-2-methylpropiophenone) 30 Visible light initiator
(mixture of acid red 94 and anilinoacetic acid) Mixing Coherent
Coherent Ultraviolet light temperature Mixing laser laser
Ultraviolet intensity Ultraviolet Post-cur- e (degrees time
wavelength time wavelength (milliwatts per light time time
Post-cure Examples Celsius) (minutes) (nanometer) (second)
(nanometer) square centimeter) (minutes) (minutes) mode 16 20 60
432 10 200 10 2 5 Ultraviolet light 17 25 57 441 15 211 20 4 10
Visible light 18 30 54 456 20 223 30 6 15 Ultraviolet light 19 35
51 462 25 245 40 8 20 Visible light 20 40 48 478 30 254 50 10 25
Ultraviolet light 21 45 45 495 35 266 60 12 30 Visible light 22 50
42 503 40 278 70 14 35 Ultraviolet light 23 55 39 512 45 288 80 16
40 Visible light 24 60 36 527 50 296 90 18 45 Ultraviolet light 25
65 33 535 12 300 100 20 50 Visible light 26 70 30 549 17 310 110 22
55 Ultraviolet light 27 75 27 553 23 325 120 24 60 Visible light 28
80 24 560 28 334 130 26 5 Ultraviolet light 29 85 21 579 31 345 140
28 10 Visible light 30 90 18 580 37 356 150 30 15 Ultraviolet
light
It should be readily understood to those skilled in the art that
the above description is only preferred embodiments of the present
disclosure, and does not limit the scope of the present disclosure.
Any change, equivalent substitution and modification made without
departing from the spirit and scope of the present disclosure
should be included within the scope of the protection of the
present disclosure.
* * * * *